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WO1996015843A1 - Azote d'une tres grande purete obtenu par separation par membrane - Google Patents

Azote d'une tres grande purete obtenu par separation par membrane Download PDF

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Publication number
WO1996015843A1
WO1996015843A1 PCT/US1995/014131 US9514131W WO9615843A1 WO 1996015843 A1 WO1996015843 A1 WO 1996015843A1 US 9514131 W US9514131 W US 9514131W WO 9615843 A1 WO9615843 A1 WO 9615843A1
Authority
WO
WIPO (PCT)
Prior art keywords
permeable
nitrogen
semi
membrane
gas
Prior art date
Application number
PCT/US1995/014131
Other languages
English (en)
Inventor
Richard A. Callahan
Kishore V. Khandavalli
Original Assignee
Enerfex, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Enerfex, Inc. filed Critical Enerfex, Inc.
Priority to EP95942391A priority Critical patent/EP0792185A4/fr
Priority to JP8516883A priority patent/JPH10509093A/ja
Publication of WO1996015843A1 publication Critical patent/WO1996015843A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/225—Multiple stage diffusion
    • B01D53/226—Multiple stage diffusion in serial connexion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/04—Purification or separation of nitrogen
    • C01B21/0405—Purification or separation processes
    • C01B21/0433—Physical processing only
    • C01B21/0438—Physical processing only by making use of membranes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0051—Carbon dioxide

Definitions

  • the present invention relates to a process for the separation and production of very high purity ( ⁇ 99.5 vol.%) nitrogen recovered from process gas streams that are predominantly (i.e., >50 vol.%) nitrogen and one or more of certain other permeable gases using an apparatus comprising one or more semi-permeable solution-diffusion membrane separation stages.
  • a separation process to produce very high purity ( 99.5 vol.%) nitrogen from a process feed gas mixture that is predominantly nitrogen, and one or more other permeable gases comprises providing said feed gas mixture under pressure to a membrane separator unit comprising a semi- permeable separation membrane with respect to which the largest fraction of the other permeable gases is at least 20 times more permeable than nitrogen, to provide a very high purity raffinate nitrogen gas product.
  • the separation factor between two gases is known as the selectivity between the gases, which is defined as the ratio of permeability of the individual gases.
  • the present invention utilizes at least a five fold higher separation factor between nitrogen and another gas constituting the largest fraction of the other permeable gases, e.g., hydrogen, carbon dioxide, or hydrogen sulfide, compared to the separation factor between nitrogen and oxygen. In many cases a relatively higher N 2 feed concentration makes the separation relatively easier and increases the productivity of the membrane separator unit.
  • FIG. 1 illustrates the process of the present invention wherein the process feed gas mixture is subjected to optional pretreatment and is separated in a membrane separator unit to produce a very high purity raffinate nitrogen gas stream.
  • Figure 2 illustrates a preferred embodiment of the process of the present invention wherein the very high purity (> 99.5 vol.%) raffinate nitrogen stream is further purified in an additional purification step to provide an ultra high purity (>99.9 vol.%) nitrogen gas product by providing the very high purity nitrogen gas product, as an intermediate product, to a second membrane separator unit comprising a second semi- permeable separation membrane having sub-atmospheric pressure on the permeate side thereof.
  • the present invention comprises a process which provides a feed gas source to recover nitrogen and a membrane separation process, where nitrogen is separated not from compositions wherein oxygen is a significant component (i.e., the 0 2 content is 5 vol.%), but rather from other gas compositions, wherein, in addition to the predominant (>50 vol.%) nitrogen, the largest fraction of the other permeable gases is a gas other than oxygen.
  • oxygen is a significant component (i.e., the 0 2 content is 5 vol.%), but rather from other gas compositions, wherein, in addition to the predominant (>50 vol.%) nitrogen, the largest fraction of the other permeable gases is a gas other than oxygen.
  • volume % volume % (vol.%) is to be understood.
  • sources such as fossil fuel combustion exhaust mainly consists of nitrogen and carbon dioxide after the removal of water.
  • Typical separation factors for C0 2 over N 2 are 20-60, which are five to ten times higher than those of 0 2 over N 2 .
  • Typical separation factors for H 2 over N 2 are 200-600, which are 50 to 100 times higher than those of 0 2 over N 2 .
  • the present invention emphasizes separating N 2 from gases such as H 2 and C0 2 instead of from 0 2 in air; this takes advantage of the higher separation factors that are typical of commercially available air separation membranes.
  • a natural gas combustion exhaust is typically comprised of 12% carbon dioxide and 88% nitrogen after removal of the water, based on the stoichiometric air-to-fuel ratio.
  • a limekiln vent gas typically contains about 79% N 2 , 20% C0 2 , and 1% 0 2 after removal of the water.
  • the higher separation factor typical for C0 2 over N 2 makes the separation much easier compared to separation of nitrogen from air.
  • smaller membrane separators are required to achieve similar purities and recoveries of N 2 compared with conventional membrane air separators.
  • nitrogen is separated from a process feed gas source 11 containing predominantly nitrogen, and carbon dioxide as the second largest fraction (i.e. , the largest fraction of the other permeable gases) , on a dry basis, taking advantage of the higher separation factors between the two primary gases, C0 2 and N 2 .
  • the separation factors reported in the literature for C0 2 over N 2 are typically between 20 and 60 for various commercially available membranes.
  • the process feed gas mixture 11, which contains N 2 and C0 2 on a dry basis is subjected to necessary pretreatment 12, such as particle removal, compression, and dehydration.
  • a process feed gas may be available at a higher temperature, a higher pressure, may contain some suspended particles, or may also contain small amounts to traces of undesirable gases such as carbon monoxide, SOX, and NOX.
  • the process gas may be water-cooled or water-scrubbed, filtered, or may even be subjected to a chemical or catalytic process before the separation.
  • the process gas feed stream is cooled in a heat exchanger using cooling water available, for example, at 85 'F, from a cooling tower or any other source. Due to the reduced temperature of the feed gas, some of the water is condensed and removed. After the water is removed, the process gas is in a saturated condition.
  • the feed gas is pressurized to about 80-200 psig in a compressor.
  • the compressed gas is again cooled in a heat exchanger, using, for example, 85 * F cooling water. Due to the change in the pressure of the process feed gas, some additional water is condensed and removed. The process gas now free of most of the water is heated to above the dew point.
  • the pressurized process feed gas 11' is then fed to the membrane separator stage 14 containing a semi-permeable membrane 16, to produce a high pressure raffinate stream 17 which is rich in nitrogen, and a permeate stream 19 rich in carbon dioxide.
  • the temperature of the feed gas entering the membrane separator stage may vary, but is typically 75-115'F, and the temperature of the two product streams are also typically 75-115'F.
  • the nitrogen purity in the raffinate is 99.5 vol.%, and the carbon dioxide content in the permeate is typically 30-50%.
  • higher purities of nitrogen in the raffinate can be achieved by passing the high pressure raffinate through a secondary membrane stage 20 using a second semi-permeable membrane 22, or using any other purification step.
  • a compressor (not shown) may be used to increase the raffinate pressure if required.
  • the raffinate nitrogen gas product 23 from a process according to the invention employing a secondary membrane typically can reach a very high purity of 99.5 vol.%, or even an ultra high purity of >99.9 vol.% nitrogen.
  • the permeate gas stream from the secondary membrane stage 25 may be recycled 27 to the feed of the first membrane separator unit by combination via 31 with process feed gas mixture 11, or, with pressurization, by combination via 33 with pressurized process feed gas 11'.
  • the feed gas mixture is a compressed feed gas stream of predominantly nitrogen, and contains carbon dioxide in a concentration of from 10% to 30 vol%.
  • a compressed non-per eate raffinate product stream which is nitrogen in a concentration of from 99.9 vol.% to 99.9995 vol%.
  • the permeate waste stream is predominantly nitrogen and has a carbon dioxide concentration of from 27.0 vol.% to 30.0 vol.%.
  • the feed gas mixture:non- permeate raffinate gas product ratio is not more than 1.8:1, to provide a product to feed recovery of at least 56% at 99.9995 vol.% nitrogen product purity.
  • the process is carried out at a production efficiency of at least 2 standard cubic feet of nitrogen per minute per compression horsepower at 99.9995 vol.% nitrogen product purity.
  • the membrane requirement per standard cubic foot of non-permeate raffinate nitrogen gas product at 99.9995 vol.% purity is less than 4/10ths that of an air separation membrane requirement per standard cubic foot at 99.5 vol.% nitrogen product purity.
  • the membrane requirement per standard cubic foot of non-permeate nitrogen product at 99.5 vol.% purity is less than 3/10ths that of an air separation membrane process at 99.5 vol.% nitrogen product purity.
  • Preferred semi-permeable separation membranes in accordance with the invention are made from at least one polymeric material selected from the group consisting of polyimide, cellulose acetate, polysulfone, polycarbonate, and polyphenylene oxide.
  • the intermediate product is provided to a second membrane separator unit comprising a second semi-permeable separation membrane having sub-atmospheric pressure on the permeate side of the second separation membrane, to thereby provide an ultra high purity raffinate nitrogen gas product.
  • a vacuum pump for the preparation of ultra high purity (>99.9 vol.%) nitrogen, after production of a very high purity raffinate nitrogen gas as an intermediate product in accordance with the basic embodiment of the invention of providing a feed gas mixture under pressure to a first membrane separator unit, the intermediate product is provided to a second membrane separator unit comprising a second semi-permeable separation membrane having sub-atmospheric pressure on the permeate side of the second separation membrane, to thereby provide an ultra high purity raffinate nitrogen gas product.
  • sub-atmospheric and sub-atmospheric pressure is preferably produced by use of a vacuum pump.
  • the second semi-permeable separation membrane such is preferably made from at least one polymeric material selected from the group consisting of polyimide, cellulose acetate, polysulfone, polycarbonate, and polyphenylene oxide.
  • the present invention describes a process to recover very high purity (>99.5 vol.%) nitrogen from a process feed gas containing predominantly nitrogen, and one or more other permeable gases, the largest fraction of which is at least 20 times more permeable than nitrogen.
  • Combustion exhaust gas and limekiln vent gas are typical examples of preferred process feed gases in accordance with the present invention.
  • the combustion exhaust example is described in detail below as a preferred embodiment.
  • a natural gas combustion exhaust gas normally contains about 9.5% C0 2 , 19% water, and 71.5% N 2 , based on the stoichiometric air-to-fuel ratio.
  • the combustion exhaust gas is normally available at atmospheric pressure and about 120-150 * F after heat recovery in an economizer.
  • this feed gas 11 is further cooled to about 95 * F in a heat exchanger using a cooling water source available, for example, at 85 * F.
  • the cooling water for the heat exchanger is supplied from a cooling tower or any other source. All of the condensed water from the cooled process gas stream is removed.
  • the process gas contains about 5.5% by volume of moisture at saturated conditions.
  • Additional drying equipment can be used to remove water to below saturated levels if the process equipment requires lower levels of moisture.
  • the treated process feed gas is then pressurized in a compressor to about 150 psig and is cooled in an after-cooler to about 95'F using 85"F cooling tower water. Water that is further condensed due to the new equilibrium conditions is removed and the saturated moisture content in the feed gas at 95'F and 150 psig is about 0.5%. Additional drying equipment further reduces water content.
  • the dried pressurized gas 11' is then supplied in a membrane separator stage 14 to a membrane 16 made of polycarbonate polymer to produce a raffinate product stream of very high purity nitrogen 17 containing 99.5 vol.% N 2 , and a permeate stream 19 containing about 30% C0 2 . Most of the remaining water in the feed stream permeates through and is present in the permeate stream.
  • the raffinate from the membrane separator is at about 140 psig and 95 * F and contains >99.5 vol.% N 2 .
  • Higher purities of N 2 can be achieved, referring to Fig. 2, by passing this raffinate stream 17 through a second membrane separator stage 20 using a second semi-permeable membrane 22, using sub- atmospheric permeate pressure, preferably by means of a vacuum pump, and preferably with recycling 27 of the permeate gas stream from the secondary membrane stage to the feed of the first membrane separator unit, or using a cryogenic purification step or other purification processes.
  • This additional purification step is cost effective because the >99.5 vol.% raffinate is already available at high pressure.
  • the equilibrium yield of ammonia is increased by increasing pressure. Temperature increase produces the opposite effect on the equilibrium, but increases the rate of reaction. Modern designs use pressures of 15 to 30 MPa at around 500'C. At these conditions the above equilibrium reaction does not go to completion and there are some unreacted reactants in the outlet of the reactor. Outlet concentrations of ammonia are 16 to 25%.
  • the outlet gases are cooled to separate ammonia from the unreacted reactants.
  • the unreacted gases are essentially a mixture of N 2 and H 2 .
  • H 2 is more permeable than N 2 , and will be collected on the permeate side of the membrane.
  • the raffinate stream containing >99.5 vol.% N 2 can be used as a product such as a blanket agent (e.g., for semiconductor manufacture, metal heat treating, etc.) or for any other useful purpose.
  • This raffinate product can also be further purified in another membrane separator to achieve even higher purities of N 2 or to make liquid nitrogen.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Ce procédé met en ÷uvre une membrane semi-perméable aux gaz afin d'obtenir de l'azote d'une très grande pureté (17) en le séparant d'un mélange de base gazeux à traiter (11). Ce mélange de base gazeux à traiter (11), composé principalement d'azote et d'autres gaz à forte capacité de pénétration, est compressé contre une unité de séparation par membrane (14) qui comporte une membrane de séparation semi-perméable (16). La majorité des autres gaz ayant une capacité de pénétration au moins 20 fois supérieure à celle de l'azote, on obtient ainsi un produit gazeux d'azote raffiné d'une très grande pureté (17).
PCT/US1995/014131 1994-11-17 1995-11-14 Azote d'une tres grande purete obtenu par separation par membrane WO1996015843A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP95942391A EP0792185A4 (fr) 1994-11-17 1995-11-14 Azote d'une tres grande purete obtenu par separation par membrane
JP8516883A JPH10509093A (ja) 1994-11-17 1995-11-14 膜分離による極高純度窒素

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US34108094A 1994-11-17 1994-11-17
US08/341,080 1994-11-17
US08/552,466 US5693121A (en) 1994-11-17 1995-11-09 Semi-permeable membrane separation process for the production of very high purity nitrogen
US08/552,466 1995-11-09

Publications (1)

Publication Number Publication Date
WO1996015843A1 true WO1996015843A1 (fr) 1996-05-30

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US1995/014131 WO1996015843A1 (fr) 1994-11-17 1995-11-14 Azote d'une tres grande purete obtenu par separation par membrane

Country Status (6)

Country Link
US (1) US5693121A (fr)
EP (1) EP0792185A4 (fr)
JP (1) JPH10509093A (fr)
KR (1) KR970706886A (fr)
CA (1) CA2205364A1 (fr)
WO (1) WO1996015843A1 (fr)

Cited By (3)

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US7008921B2 (en) 2000-09-05 2006-03-07 Karolinska Innovations Ab Materials and methods relating to endothelial cell growth inhibitors
WO2008134009A3 (fr) * 2007-04-27 2010-01-14 Nitro-Lift Technologies, Inc. Générateurs d'azote non cryogènes et procédés d'utilisation
FR2962994A1 (fr) * 2010-07-20 2012-01-27 Air Liquide Procede de production d’un flux riche en azote

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US7765794B2 (en) * 2001-05-04 2010-08-03 Nco2 Company Llc Method and system for obtaining exhaust gas for use in augmenting crude oil production
US6893615B1 (en) * 2001-05-04 2005-05-17 Nco2 Company Llc Method and system for providing substantially water-free exhaust gas
US20070012182A1 (en) * 2005-07-18 2007-01-18 Ingersoll-Rand Company Fluid distribution system and method of operating the same
DE102007020625A1 (de) * 2007-04-30 2008-11-06 Khs Ag Verfahren zum Verarbeiten, insbesondere zum Verpacken von Produkten unter Verwendung eines sauerstofffreien Prozessgases
CN101481101B (zh) * 2008-01-09 2011-04-20 中国石油化工股份有限公司 一种用膜回收烟气中氮气的方法
CN101480559B (zh) * 2008-01-09 2011-04-20 中国石油化工股份有限公司 一种用膜回收烟气中硫的方法
US8114191B2 (en) * 2008-12-11 2012-02-14 General Electric Company Energy efficient approach to CO2 capture process
FR2942934B1 (fr) * 2009-03-09 2011-10-21 Eurocopter France Procede pour appliquer un produit electriquement conducteur, liquide lors de son application, sur un support afin de relier deux elements electriquement conducteurs.
KR102235015B1 (ko) * 2019-04-26 2021-04-02 (주)에어레인 연소배가스를 이용한 질소농축공기의 제조방법
CN110885068B (zh) * 2019-12-23 2024-08-20 南通广兴气动设备有限公司 一种便携式高压制氮气机

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7008921B2 (en) 2000-09-05 2006-03-07 Karolinska Innovations Ab Materials and methods relating to endothelial cell growth inhibitors
WO2008134009A3 (fr) * 2007-04-27 2010-01-14 Nitro-Lift Technologies, Inc. Générateurs d'azote non cryogènes et procédés d'utilisation
FR2962994A1 (fr) * 2010-07-20 2012-01-27 Air Liquide Procede de production d’un flux riche en azote

Also Published As

Publication number Publication date
US5693121A (en) 1997-12-02
KR970706886A (ko) 1997-12-01
JPH10509093A (ja) 1998-09-08
EP0792185A4 (fr) 1998-04-15
CA2205364A1 (fr) 1996-05-30
EP0792185A1 (fr) 1997-09-03

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